CN108816218A - Modified vanadium series catalyst of a kind of Mn oxide for exhaust gas from diesel vehicle denitration and its preparation method and application - Google Patents
Modified vanadium series catalyst of a kind of Mn oxide for exhaust gas from diesel vehicle denitration and its preparation method and application Download PDFInfo
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- CN108816218A CN108816218A CN201810712845.1A CN201810712845A CN108816218A CN 108816218 A CN108816218 A CN 108816218A CN 201810712845 A CN201810712845 A CN 201810712845A CN 108816218 A CN108816218 A CN 108816218A
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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Abstract
The present invention relates to modified vanadium series catalysts of a kind of Mn oxide for exhaust gas from diesel vehicle denitration and its preparation method and application.The preparation method includes the following steps：S1：By manganese acetylacetonate（III）Dissolution obtains manganese precursor solution；S2：Vanadium series catalyst is added into the manganese precursor solution, is stirred, is roasted in air atmosphere after dry and obtains the modified vanadium series catalyst of Mn oxide；In the modified vanadium series catalyst of the Mn oxide, the mass fraction of Mn oxide is 0.03 ~ 0.08%.It is preparation method simplicity provided by the invention, easy controlled operation, reproducible；The modified vanadium series catalyst of the Mn oxide that is prepared has higher denitration activity, and temperature window has widened 40 DEG C, and conversion rate of NOx in the range of 255 ~ 465 DEG C reaches 90% or more, can wide popularization and application in exhaust gas from diesel vehicle denitration process.
Description
Technical field
The invention belongs to catalysis material preparation fields, and in particular to a kind of Mn oxide for exhaust gas from diesel vehicle denitration changes
Property vanadium series catalyst and its preparation method and application.
Background technique
In recent years, with the rapid development of China Transportation Industry, atmosphere pollution caused by automotive emission causes
The great attention of country.
Compared to gasoline car, diesel vehicle reduces carbon monoxide in tail gas using the technology of optimization burning（CO）With hydrocarbonization
Close object（HCs）Discharge, but nitrogen oxides（NOx）Discharge amount be much higher than gasoline car.NOx can cause haze weather, can also make
At photochemical fog, human health is seriously endangered.Selective catalytic reduction（Selective Catalytic Reduction,
SCR）Technology has been found to be one of most effective diesel vehicle denitration technology.SCR denitration technology is generally also with NH3, hydro carbons etc.
Former agent, is reduced to N2 for NOx under the effect of the catalyst.In addition to exhaust gas from diesel vehicle denitration field, this denitration technology is also extensive
For thermal power plant, boiler, coke-oven plant etc..
The type of denitration effect and used catalyst is closely related.From 1970s, vanadium series catalyst starts for diesel vehicle
Tail gas denitration.Traditional vanadium series catalyst is generally with TiO2For carrier, V2O5For active component, and with WO3Or MoO3It is helped for catalysis
Agent enhances the anti-caking power of catalyst.This catalyst generally has a preferable denitration activity at 300 ~ 400 DEG C, and have compared with
Up to the present high stability and cheap price are still the most widely used denitrating catalyst of industry.However, with country
The further upgrading of emission regulation needs that traditional vanadium series catalyst is optimized or found new catalysis material and comes further
Meet national emission request.
Summary of the invention
It is an object of the invention to overcome vanadium series catalyst traditional in the prior art nothing in vehicle exhaust denitration process
Method meets the defect and deficiency of national emission request, provides a kind of modified vanadium system of the Mn oxide for exhaust gas from diesel vehicle denitration and urges
The preparation method of agent.It is preparation method simplicity provided by the invention, easy controlled operation, reproducible；The Mn oxide being prepared
Modified vanadium series catalyst has higher denitration activity, and temperature window has widened 40 DEG C, NOx in the range of 255 ~ 465 DEG C
Conversion ratio reaches 90% or more, can wide popularization and application in exhaust gas from diesel vehicle denitration process.
Another object of the present invention is to provide a kind of modified vanadium series catalysts of Mn oxide.
Another object of the present invention is to provide the modified vanadium series catalysts of above-mentioned Mn oxide in exhaust gas from diesel vehicle denitration
Application.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of the modified vanadium series catalyst of Mn oxide for exhaust gas from diesel vehicle denitration, includes the following steps：
S1：By manganese acetylacetonate（III）Dissolution obtains manganese precursor solution；
S2：Vanadium series catalyst is added into the manganese precursor solution, is stirred, roasts in air atmosphere after dry and obtains
Mn oxide is modified vanadium series catalyst；In the modified vanadium series catalyst of the Mn oxide, the mass fraction of Mn oxide is 0.03 ~
0.08%。
The present inventor has found after study, when being modified to vanadium series catalyst, on the one hand, is aoxidized by incorporation
Object is the most directly, effectively come the low-temperature denitration activity and operation window for improving vanadium series catalyst；On the other hand, Mn oxide
With valence state abundant and good low-temperature reduction, it can promote NO and be oxidized to NO2, the reaction rate of SCR is improved, is suitable for conduct
Modified material.
Preparation method provided by the invention is carried out by loading low concentration Mn oxide in conventional vanadium series catalyst
Modified, the modified vanadium series catalyst of obtained Mn oxide has higher denitration activity, and temperature window has widened 40 DEG C, 255 ~
Conversion rate of NOx in the range of 465 DEG C reaches 90% or more, can wide popularization and application in exhaust gas from diesel vehicle denitration process.
Preparation method provided by the invention only need to it is original prepare vanadium series catalyst process flow on the basis of repeat a step
Load the operation of low concentration Mn oxide, it is simple process, easy controlled operation, reproducible, it can be widely used for being catalyzed existing vanadium system
Agent carries out large-scale optimization and is modified.
Preferably, it is acetone that selected solvent is dissolved in S1.
The present invention selects manganese acetylacetonate（III）As manganese precursor salt, the acetone small using volatile, surface tension is as molten
Agent effectively prevents Mn caused by capillary effect in the drying process3+In the enrichment of catalyst channel surfaces, Mn is improved3+'s
Dispersion degree.
Preferably, in the modified vanadium series catalyst of the Mn oxide, the mass fraction of Mn oxide is 0.05%.
It in order to be better mixed uniformly, and is easily dried, it is preferable that vanadium series catalyst is added to the manganese presoma in S2
When in solution, the manganese precursor solution soaks the vanadium series catalyst.
It should be understood that the amount of manganese precursor solution soaks vanadium series catalyst, it is unsuitable excessive.
Preferably, process dry in S2 is：After natural drying, dry 8 ~ 12h under the conditions of 60 ~ 80 DEG C.
Routine vanadium series catalyst in the prior art is used equally in the present invention, is modified to it.
Preferably, vanadium series catalyst described in S2 is with TiO2For carrier, V2O5For active component, WO3For auxiliary agent.
It is further preferable that in the modified vanadium series catalyst of the Mn oxide, V2O5Mass fraction be 1 ~ 5 %, WO3Matter
Amount score is 1 ~ 10 %, TiO2Mass fraction be 80 ~ 98 %.
The present invention provides a kind of method for preparing conventional vanadium series catalyst.
Preferably, the vanadium series catalyst is prepared via a method which to obtain：
S001：By carrier titanium dioxide TiO23 ~ 5h is roasted in 300 ~ 400 DEG C of air atmosphere；
S002：Ammonium metavanadate, ammonium metatungstate and oxalic acid solution are mixed, after S001 roasting is added to after being completely dissolved for stirring
TiO2, stir, 2 ~ 5h roasted after dry in 400 ~ 600 DEG C of air atmosphere to get the vanadium series catalyst is arrived.
Preferably, the TiO after being roasted in S0012Crystal form be anatase.
Preferably, the time roasted in S001 is 4h.
Preferably, the concentration of oxalic acid solution described in S002 is 0.1 ~ 0.5 mol/L.
Preferably, TiO is added in S0022When, the mixed solution soaks the TiO2。
It should be understood that the amount of mixed solution soaks TiO2, unsuitable excessive.
Preferably, the temperature roasted in S002 is 450 ~ 550 DEG C, and the time of roasting is 2 ~ 5h.
A kind of modified vanadium series catalyst of Mn oxide, is prepared by above-mentioned preparation method.
Application of the modified vanadium series catalyst of above-mentioned Mn oxide in exhaust gas from diesel vehicle denitration is also in protection model of the invention
In enclosing.
Compared with prior art, the present invention has the advantages that：
It is preparation method simplicity provided by the invention, easy controlled operation, reproducible；The modified vanadium system catalysis of the Mn oxide being prepared
Agent has higher denitration activity, and temperature window has widened 40 DEG C, and conversion rate of NOx in the range of 255 ~ 465 DEG C reaches 90%
More than, can wide popularization and application in exhaust gas from diesel vehicle denitration process.
Detailed description of the invention
Fig. 1 is the SCR activity test result for the catalyst that the embodiment of the present invention 1 ~ 3 is prepared；
The SCR activity test result for the catalyst that Fig. 2 is the embodiment of the present invention 1, comparative example 1 ~ 3 is prepared；
Fig. 3 is the X-ray diffractogram of the embodiment of the present invention 1；
Fig. 4 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of modified vanadium series catalyst V of Mn oxide for exhaust gas from diesel vehicle denitration2O5-WO3-MnOx/
TiO2- 1, the method for being prepared by the following procedure is prepared.
Prepare V2O5-WO3-MnOx/TiO2-1：（1）By carrier TiO2Roasting 3 ~ 5 is small in 300 ~ 400 DEG C of air atmosphere
When Removal of catalyst duct in moisture and foreign gas.A certain amount of ammonium metavanadate and ammonium metatungstate are taken, it is 0.1 that concentration, which is added,
The oxalic acid solution of ~ 0.5 mol/L is stirred to it and is completely dissolved.Using equi-volume impregnating, by the pretreated carrier of step
TiO2It is added in the solution of the above-mentioned preparation of step, stirs 0.5 hour, spontaneously dry, then dry 8 ~ 12 under the conditions of 60 ~ 80 DEG C
Hour.Powder after drying is roasted 2 ~ 5 hours in 400 ~ 600 DEG C of air atmosphere, obtains vanadium series catalyst.（2）Using
Equi-volume impregnating, by the manganese acetylacetonate of obtained vanadium series catalyst addition acetone solution（III）In solution, 10 points are stirred
Clock spontaneously dries, then 8 ~ 12 hours dry under the conditions of 60 ~ 80 DEG C.Powder after drying roasts in 550 DEG C of air atmosphere
It burns 4 hours, obtains the modified vanadium series catalyst of Mn oxide.Wherein, active component V2O5The mass percent for accounting for catalyst is 3
%, auxiliary agent WO3The mass percent for accounting for catalyst is 10 %, MnOxThe mass percent for accounting for catalyst is 0.05%, carrier TiO2It accounts for
The mass percent of catalyst is about 86.95 %.
Embodiment 2
The present embodiment provides a kind of modified vanadium series catalyst V of Mn oxide for exhaust gas from diesel vehicle denitration2O5-WO3-MnOx/
TiO2, the method for being prepared by the following procedure is prepared.
Select step in embodiment 1（1）Vanadium series catalyst is prepared, using equi-volume impregnating, the vanadium system that will be obtained
The manganese acetylacetonate for using acetone solution is added in catalyst（III）It in solution, stirs 10 minutes, spontaneously dries, then at 60 ~ 80 DEG C
Under the conditions of dry 8 ~ 12 hours.Powder after drying roasts 4 hours in 550 DEG C of air atmosphere, and it is modified to obtain Mn oxide
Vanadium series catalyst.Wherein, active component V2O5The mass percent for accounting for catalyst is 3 %, auxiliary agent WO3Account for the quality of catalyst
Percentage is 10 %, MnOxThe mass percent for accounting for catalyst is 0.03%, carrier TiO2The mass percent for accounting for catalyst is about
86.97 %。
Embodiment 3
The present embodiment provides a kind of modified vanadium series catalyst V of Mn oxide for exhaust gas from diesel vehicle denitration2O5-WO3-MnOx/
TiO2, the method for being prepared by the following procedure is prepared.
Select step in embodiment 1（1）Vanadium series catalyst is prepared, using equi-volume impregnating, the vanadium system that will be obtained
The manganese acetylacetonate for using acetone solution is added in catalyst（III）It in solution, stirs 10 minutes, spontaneously dries, then at 60 ~ 80 DEG C
Under the conditions of dry 8 ~ 12 hours.Powder after drying roasts 4 hours in 550 DEG C of air atmosphere, and it is modified to obtain Mn oxide
Vanadium series catalyst.Wherein, active component V2O5The mass percent for accounting for catalyst is 3%, auxiliary agent WO3Account for the quality hundred of catalyst
Divide than being 10 %, MnOxThe mass percent for accounting for catalyst is 0.08%, carrier TiO2The mass percent for accounting for catalyst is about
86.92 %。
Comparative example 1
This comparative example provides a kind of conventional vanadium series catalyst, in preparation method and embodiment 1（1）Unanimously, specific as follows.
Prepare V2O5-WO3/TiO2：By carrier TiO24 hours Removal of catalyst are roasted in 300 ~ 400 DEG C of air atmosphere
Moisture and foreign gas in duct.A certain amount of ammonium metavanadate and ammonium metatungstate are taken, it is 0.1 ~ 0.5 mol/L's that concentration, which is added,
Oxalic acid solution is stirred to it and is completely dissolved.Using equi-volume impregnating, by the pretreated carrier TiO of step2It is added in step
It states in the solution of preparation, stirs 0.5 hour, spontaneously dry, it is then 8 ~ 12 hours dry under the conditions of 60 ~ 80 DEG C.After dry
Powder roasted 2 ~ 5 hours in 400 ~ 600 DEG C of air atmosphere, obtain vanadium series catalyst.Wherein, active component V2O5It accounts for and urges
The mass percent of agent is 3 %, auxiliary agent WO3The mass percent for accounting for catalyst is 10 %, carrier TiO2Account for the quality of catalyst
Percentage is 87 %.
Comparative example 2
The present embodiment provides a kind of modified vanadium series catalyst V of Mn oxide for loading high concentration manganese oxide2O5-WO3-MnOx/
TiO2-2.It is prepared via a method which to obtain.
Prepare V2O5-WO3-MnOx/TiO2-2：（1）By carrier TiO2It is roasted 4 hours in 300 ~ 400 DEG C of air atmosphere
Moisture and foreign gas in Removal of catalyst duct.Take a certain amount of ammonium metavanadate and ammonium metatungstate, be added concentration be 0.1 ~
The oxalic acid solution of 0.5 mol/L is stirred to it and is completely dissolved.Using equi-volume impregnating, by the pretreated carrier of step
TiO2It is added in the solution of the above-mentioned preparation of step, stirs 0.5 hour, spontaneously dry, then dry 8 ~ 12 under the conditions of 60 ~ 80 DEG C
Hour.Powder after drying is roasted 2 ~ 5 hours in 400 ~ 600 DEG C of air atmosphere, obtains vanadium series catalyst.（2）Using
Equi-volume impregnating, by the manganese acetylacetonate of obtained vanadium series catalyst addition acetone solution（III）In solution, 10 points are stirred
Clock spontaneously dries, then 8 ~ 12 hours dry under the conditions of 60 ~ 80 DEG C.Powder after drying roasts in 550 DEG C of air atmosphere
It burns 4 hours, obtains the modified vanadium series catalyst of Mn oxide.Wherein, active component V2O5The mass percent for accounting for catalyst is 3
%, auxiliary agent WO3The mass percent for accounting for catalyst is 10 %, MnOxThe mass percent for accounting for catalyst is 0.5%, carrier TiO2It accounts for
The mass percent of catalyst is about 86.5 %
Comparative example 3
The present embodiment provides a kind of modified vanadium series catalyst V of Mn oxide for loading high concentration manganese oxide2O5-WO3-MnOx/
TiO2-3.It is prepared via a method which to obtain.
Prepare V2O5-WO3-MnOx/TiO2-3：（1）By carrier TiO2It is roasted 4 hours in 300 ~ 400 DEG C of air atmosphere
Moisture and foreign gas in Removal of catalyst duct.Take a certain amount of ammonium metavanadate and ammonium metatungstate, be added concentration be 0.1 ~
The oxalic acid solution of 0.5 mol/L is stirred to it and is completely dissolved.Using equi-volume impregnating, by the pretreated carrier of step
TiO2It is added in the solution of the above-mentioned preparation of step, stirs 0.5 hour, spontaneously dry, then dry 8 ~ 12 under the conditions of 60 ~ 80 DEG C
Hour.Powder after drying is roasted 2 ~ 5 hours in 400 ~ 600 DEG C of air atmosphere, obtains vanadium series catalyst.（2）Using
Equi-volume impregnating, by the manganese acetylacetonate of obtained vanadium series catalyst addition acetone solution（III）In solution, 10 points are stirred
Clock spontaneously dries, then 8 ~ 12 hours dry under the conditions of 60 ~ 80 DEG C.Powder after drying roasts in 550 DEG C of air atmosphere
It burns 4 hours, obtains the modified vanadium series catalyst of Mn oxide.Wherein, active component V2O5The mass percent for accounting for catalyst is 3
%, auxiliary agent WO3The mass percent for accounting for catalyst is 10 %, MnOxThe mass percent for accounting for catalyst is 2 %, carrier TiO2It accounts for and urges
The mass percent of agent is about 85 %.
Catalyst prepared by above-described embodiment 1 ~ 3 and embodiment 1, comparative example 1 ~ 3 is in 84000 h of air speed-1, 500 ppm
NO, 500 ppm NH3, 5%O2Under conditions of test, test result difference it is as illustrated in fig. 1 and 2.From figure 1 it appears that implementing
The activity of example 1 ~ 3 is not much different, and the denitration activity of catalyst is best when Mn oxide load capacity is 0.05% in embodiment 1.By scheming
2 it is found that the temperature window of embodiment 1 has widened 40 DEG C compared to comparative example 1, NO in the range of 255 ~ 465 DEG CxConversion
Rate reaches 90% or more, and apparent advantage is embodied in denitration activity.In addition, denitration of the load capacity of Mn oxide to catalyst
Activity plays an important role.By the active testing result of comparative example 2,3 it is found that with Mn oxide load capacity increase, change
Decrease with the obvious advantage in property catalyst denitration activity, even lower than unmodified catalyst.
Claims (10)
1. a kind of preparation method of the modified vanadium series catalyst of Mn oxide for exhaust gas from diesel vehicle denitration, which is characterized in that packet
Include following steps：
S1：By manganese acetylacetonate（III）Dissolution obtains manganese precursor solution；
S2：Vanadium series catalyst is added into the manganese precursor solution, is stirred, roasts in air atmosphere after dry and obtains
Mn oxide is modified vanadium series catalyst；In the modified vanadium series catalyst of the Mn oxide, the mass fraction of Mn oxide is 0.03 ~
0.08%。
2. preparation method according to claim 1, which is characterized in that dissolving selected solvent in S1 is acetone.
3. preparation method according to claim 1, which is characterized in that in the modified vanadium series catalyst of the Mn oxide, manganese oxygen
The mass fraction of compound is 0.05%.
4. preparation method according to claim 1, which is characterized in that vanadium series catalyst is described in S2 with TiO2For carrier, V2O5
For active component, WO3For auxiliary agent.
5. preparation method according to claim 4, which is characterized in that in the modified vanadium series catalyst of the Mn oxide, V2O5's
Mass fraction is 1 ~ 5 %, WO3Mass fraction be 1 ~ 10 %, TiO2Mass fraction be 80 ~ 98 %.
6. preparation method according to claim 1, which is characterized in that the vanadium series catalyst is prepared via a method which
It arrives：
S001：By carrier titanium dioxide TiO23 ~ 5h is roasted in 300 ~ 400 DEG C of air atmosphere；
S002：Ammonium metavanadate, ammonium metatungstate and oxalic acid solution are mixed, stirs to mixed solution is completely dissolved to obtain, is then added
TiO after S001 roasting2, stirring, 2 ~ 5h of roasting urges in 400 ~ 600 DEG C of air atmosphere to get to the vanadium system after drying
Agent.
7. preparation method according to claim 4, which is characterized in that the TiO after being roasted in S0012Crystal form be anatase.
8. preparation method according to claim 1, which is characterized in that the temperature roasted in S002 is 450 ~ 650 DEG C, roasting
Time is 2 ~ 5h.
9. a kind of modified vanadium series catalyst of Mn oxide, which is characterized in that pass through any preparation method system of claim 1 ~ 8
It is standby to obtain.
10. application of the modified vanadium series catalyst of any Mn oxide of claim 1 ~ 9 in exhaust gas from diesel vehicle denitration.
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| CN113559846A (en) * | 2021-07-28 | 2021-10-29 | 苏州西热节能环保技术有限公司 | SCR catalyst modification method for removing flue gas chlorobenzene by catalytic combustion and catalyst |
| CN113877566A (en) * | 2021-09-23 | 2022-01-04 | 安徽元琛环保科技股份有限公司 | Preparation method of SCR denitration catalyst for preventing heavy metal poisoning and prepared SCR denitration catalyst |
| CN113877566B (en) * | 2021-09-23 | 2024-01-19 | 安徽元琛环保科技股份有限公司 | Preparation method of SCR denitration catalyst for preventing heavy metal poisoning and prepared SCR denitration catalyst |
| CN114192158A (en) * | 2021-12-30 | 2022-03-18 | 山东大学 | Preparation method of CO and NOx synergistic removal catalyst |
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